CN107727767A - The method of styrene and acrylonitrile content in translocation workplace air - Google Patents
The method of styrene and acrylonitrile content in translocation workplace air Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
- G01N30/6073—Construction of the column body in open tubular form
- G01N30/6078—Capillaries
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
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Abstract
The present invention relates to a kind of method of styrene and acrylonitrile content in translocation workplace air.The method of styrene and acrylonitrile content is determined using capillary chromatography in the translocation workplace air, is comprised the following steps：Standard liquid is prepared, sample is gathered, prepares sample solution, the standard liquid is determined and draws standard curve and the measure sample solution；Wherein, the chromatographic condition of the capillary chromatography measure is：Capillary chromatographic column is polarity capillary column；Using split sampling mode, split ratio 20: 1, the bypass flow is 30mL/min；The column flow is 1.5mL/min, and the make-up gas flow is 5mL/min, and the sample size is 1.0 μ L；The injector temperature is 230 DEG C, and the detector temperature is 250 DEG C；The initial column temperature is 40 DEG C, keeps 2min, column temperature is warming up to 60 DEG C with 5 DEG C/min heating rate, then is warming up to 90 DEG C with 15 DEG C/min heating rate, is finally warming up to 140 DEG C with 25 DEG C/min heating rate.This method is easy to operate, and detection efficiency is high.
Description
Technical field
The present invention relates to technical field of analysis and detection, more particularly to styrene and third in a kind of translocation workplace air
The method of alkene nitrile content.
Background technology
Acrylonitritrile-styrene resin (AS resins) is moulded by acrylonitrile and the styrene copolymerized engineering thermoplastic formed
Material, has excellent heat resistance, solvent resistance and good mechanical performance, is widely used in processing machinery part, meter housing, instrument
The products such as disk, battery case, automotive oil tank, battery cell case, packing container, commodity.
AS resins are processed generally by Shooting Technique, and its fusion temperature is 200 DEG C -270 DEG C.In AS resins
Hot injection moulding process in acrylonitrile monemer and styrene monomer can be diffused into the air of workplace, and national clear stipulaties third
Alkene nitrile monomer and styrene monomer are the noxious material in workplace air.In order to ensure worker health, create safe
Working condition and working environment, state compulsion require the content of styrene and acrylonitrile in measure workplace air.
The method that the content of styrene and acrylonitrile in workplace air is determined in conventional art is to styrene and third
Alkene nitrile samples respectively, then individually tests and analyzes, and its operating process is cumbersome, analysis time length, and detection efficiency is low.
The content of the invention
Based on this, it is necessary to provide it is a kind of easy to operate, in the high translocation workplace air of detection efficiency styrene and
The method of acrylonitrile content.
A kind of method of styrene and acrylonitrile content in translocation workplace air, is determined with capillary chromatography, bag
Include following steps：Standard liquid is prepared, sample is gathered, prepares sample solution, determine the standard liquid and draw standard curve
And the measure sample solution；
Wherein, the chromatographic condition of the capillary chromatography measure is：Capillary chromatographic column is polarity capillary column；Detection
Device is hydrogen flame ionization detector；Using split sampling mode, split ratio 20: 1, the bypass flow is 30mL/min；Institute
It is 1.5mL/min to state column flow, and the make-up gas flow is 5mL/min, and the sample size is 1.0 μ L；The injector temperature
For 230 DEG C, the detector temperature is 250 DEG C；The initial column temperature is 40 DEG C, keeps 2min, column temperature is with 5 DEG C/min heating
Speed is warming up to 60 DEG C, then is warming up to 90 DEG C with 15 DEG C/min heating rate, is finally heated up with 25 DEG C/min heating rate
To 140 DEG C.
In wherein one is implemented, the carrier gas of the capillary chromatography is high pure nitrogen.
In wherein one is implemented, the polarity capillary column is FFAP polarity capillary columns.
In wherein one is implemented, model 30m × 0.32mm × 1.0 μm of the FFAP polarity capillary column.
In wherein one is implemented, described the step of preparing standard liquid, includes：5ml stripping liquids are added to 10ml parsings
In bottle, 10mg styrene chromatographically pure is weighed respectively and 2mg acrylonitrile chromatographically pures are added in the parsing bottle, it is dilute to add stripping liquid
Release to scale, prepare obtain 1000 μ g/mL polystyrene standards solution and 200 μ g/mL acrylonitrile standard liquid respectively.
In wherein one is implemented, described the step of gathering sample, includes：
The step of collection sample, includes：Activated carbon tube is connected with air sampler, and activity is opened in sampled point
Charcoal pipe both ends, sampled by the short time, sampling for a long time or personal sampling gather air sample；Again by the activated carbon tube and institute
Air sampler separation is stated, to gather sample blank；The complete closing activated carbon tube both ends, are placed in cleaning container after the completion of sampling
Interior transport and preservation；Wherein, the step of short time sampling includes：The both ends of the activated carbon tube are opened in sampled point, will
The activated carbon tube is connected with the air sampler, with 100ml/min flow collection 15min air samples；The long-time
The step of sampling, includes：The both ends of the activated carbon tube are opened in sampled point, by the activated carbon tube and the air sampler
It is connected, with 50ml/min flow collection 2h-8h air samples；The step of personal sampling, includes：Described in being opened in sampled point
The both ends of activated carbon tube, the activated carbon tube is connected with the air sampler, the shirtfront top of sample objects is worn on, connects
Nearly breathing zone, with 50ml/min flow collection 2h-8h air samples；The step of collection sample blank, includes：In sampled point
The both ends of the activated carbon tube are opened, Activated charcoal tube is not connected to the air sampler, the sampling of remaining step and the short time,
The step of long-time sampling or the personal sampling, is identical.
In wherein one is implemented, the sample solution includes air sample solution and sample blank solution；Described in preparation
The step of air sample solution, includes：The both ends for the Activated charcoal tube for gathering air sample are poured into parsing bottle respectively, added
Enter stripping liquid, closing shaking, produce air sample solution；The both ends for the Activated charcoal tube for gathering sample blank are poured into respectively
Parse in bottle, add stripping liquid, closing shaking, produce sample blank solution.
It is described to determine the standard liquid and include the step of drawing standard curve in wherein one is implemented：By described in
Standard liquid is injected into the capillary chromatography and is measured, and is repeated three times, respectively obtain corresponding peak height value or
Peak area value, mark is drawn to corresponding concentration of styrene or the fine content of propylene with the peak height value or the average of peak area value respectively
Directrix curve.
In wherein one is implemented, it is molten including measure air sample solution and determination sample blank to determine the sample solution
Liquid, specific steps include：Using with determining the standard liquid identical condition determination, respectively by the air sample solution and
The sample blank solution is injected into the capillary chromatography and is measured, respectively obtain the air sample peak height value or
The peak height value or peak area value of peak area value and the sample blank, it is empty that the peak height value of the air sample is subtracted into the sample
White peak height value, or the peak area value of the air sample is subtracted to the peak area value of the sample blank, obtained by standard curve
Benzene in air ethene or the fine content of propylene.
In the translocation workplace air of the present invention capillary chromatography is used in the method for styrene and acrylonitrile content
Measure, its capillary chromatographic column is polarity capillary column, and detector is hydrogen flame ionization detector, and by adjusting chromatostrip
Part, styrene and acrylonitrile that can simultaneously in the air of collecting work place, and its content can be measured simultaneously.This method is simple
Convenient, detection efficiency is high, and complies with the national standard requirements.Styrene and third in the workplace air detected by this method
The content of alkene nitrile, time-saving and efficiency, data are accurate, and enterprise can be instructed to carry out prevention and control of occupational disease, reduce the hair of occupational disease
Sick rate, it is ensured that safety in production.
Brief description of the drawings
Fig. 1 is the chromatogram of styrene and acrylonitrile in workplace air in an embodiment.
Embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In accompanying drawing
Give presently preferred embodiments of the present invention.But the present invention can realize in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is to make the understanding to the disclosure more thorough
Comprehensively.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
The arbitrary and all combination of the Listed Items of pass.
The method of styrene and acrylonitrile content in the translocation workplace air, is determined using capillary chromatography, tool
Body comprises the following steps：Standard liquid is prepared, sample is gathered, prepares sample solution, the standard liquid is determined and draws standard song
Line and determine the sample solution.
The capillary chromatographic column of the capillary chromatography is polarity capillary column.Alternatively, the polarity capillary column is
FFAP polarity capillary columns.Still optionally further, model 30m × 0.32mm × 1.0 μm of the FFAP polarity capillary columns.Inspection
Survey device is hydrogen flame ionization detector.Alternatively, the carrier gas of the capillary chromatography is high pure nitrogen.
The chromatographic condition of capillary chromatography measure uses split sampling mode, split ratio 20: 1, the shunting stream
Measure as 30mL/min；The column flow is 1.5mL/min, and the make-up gas flow is 5mL/min, and the sample size is 1.0 μ L；
The injector temperature is 230 DEG C, and the detector temperature is 250 DEG C；Column temperature is heated up using three ranks：1) 40 DEG C of initial temperature, keep
2min；2) 60 DEG C are risen to 5 DEG C/min heating rate, keeps 0min；3) 90 DEG C are risen to 15 DEG C/min heating rate, protected
Hold 0min；4) 140 DEG C are risen to 25 DEG C/min heating rate, keeps 0min.
The method of styrene and acrylonitrile content in the translocation workplace air, specifically comprises the following steps：
1) standard liquid is prepared
5ml stripping liquids are added in 10ml parsing bottles, weigh about 10mg styrene chromatographically pure and about 2mg acrylonitrile respectively
Chromatographically pure is added in the parsing bottle, is added stripping liquid and is diluted to scale, preparation obtains about 1000 μ g/mL polystyrene standards
The acrylonitrile standard liquid of solution and 200 μ g/mL.
2) sample is gathered
Activated carbon tube is connected with air sampler, and activated carbon tube both ends are opened in sampled point, sampled by the short time,
Sampling for a long time or personal sampling collection air sample.The activated carbon tube is separated with the air sampler again, to gather sample
Blank；Complete closing activated carbon tube both ends after the completion of sampling, it is placed in transport in cleaning container and preserves.
Wherein, the step of short time samples includes：The activated carbon tube is connected with the air sampler, beaten in sampled point
Activated carbon tube both ends are opened, with 100ml/min flow collection 15min air samples.The step of long-time samples includes：This is lived
Property charcoal pipe be connected with the air sampler, activated carbon tube both ends are opened in sampled point, with 50ml/min flow collection 2h-8h air
Sample.The step of personal sampling, includes：The activated carbon tube is connected with the air sampler, activated carbon tube is opened in sampled point
Both ends, the shirtfront top of sample objects is worn on, close to breathing zone, with 50ml/min flow collection 2h-8h air samples.This is adopted
The step of collecting sample blank includes：The Activated charcoal tube is not connected to the air sampler, remaining step and short time sampling, the length
The step of time sampling or personal sampling, is identical.
3) sample solution is prepared
The sample solution includes air sample solution and sample blank solution.The Activated charcoal tube of air sample will be gathered
Both ends are poured into parsing bottle respectively, are added stripping liquid, closing shaking, are produced air sample solution.Being somebody's turn to do for sample blank will be gathered
The both ends of Activated charcoal tube are poured into parsing bottle respectively, are added stripping liquid, closing shaking, are produced sample blank solution.
4) determine the standard liquid and draw standard curve
The standard liquid is injected into the capillary chromatography to be measured, is repeated three times, is respectively obtained corresponding
Peak height value or peak area value, contain so that the peak height value or the average of peak area value are fine to corresponding concentration of styrene or propylene respectively
Amount draws standard curve.The peak height value or the average of peak area value be exactly by determine respectively obtain three times corresponding peak height value or
The average value of peak area value.
5) determination sample solution
Determining the sample solution includes measure air sample solution and determination sample blank solution.Using with determining the standard
Solution identical condition determination, the air sample solution and the sample blank solution are injected into the capillary chromatography respectively and entered
Row measure, respectively obtain the peak height value or the peak height value or peak area value of peak area value and the sample blank of the air sample.Will
The peak height value of the air sample subtracts the peak height value of the sample blank, or the peak area value of the air sample is subtracted into sample sky
White peak area value, styrene in air or the fine content of propylene are obtained by standard curve.
In the translocation workplace air of the present invention capillary chromatography is used in the method for styrene and acrylonitrile content
Measure, its capillary chromatographic column is polarity capillary column, and detector is hydrogen flame ionization detector, and by adjusting chromatostrip
Part, styrene and acrylonitrile that can simultaneously in the air of collecting work place, and its content can be measured simultaneously.This method is simple
Convenient, detection efficiency is high, and complies with the national standard requirements.Styrene and third in the workplace air detected by this method
The content of alkene nitrile, time-saving and efficiency, data are accurate, and enterprise can be instructed to carry out prevention and control of occupational disease, reduce the hair of occupational disease
Sick rate, it is ensured that safety in production.
Specific embodiment
Embodiment 1
The method 1 of styrene and acrylonitrile content in translocation workplace air
1st, instrument and test drug
1.1 capillary chromatographies, attached hydrogen flame ionization detector.
1.2 balances, ± 0.01mg
1.3 activated carbon tubes, solvent desorption type, built-in 100mg/50mg activated carbons.
1.4 air samplers, flow 0ml/min-500ml/min.
1.5 solvent desorption bottles, 5ml.
1.6 micro syringes, 10ml.
1.7 styrene, acrylonitrile chromatographically pure.
1.8 chromatographic condition：
Capillary chromatographic column：FFAP polarity capillary columns, specification are 30m × 0.32mm × 1.0 μm.
Detector：Hydrogen flame ionization detector, carrier gas high pure nitrogen.
Input mode：Split sampling, split ratio 20: 1, bypass flow 30mL/min.
Sample size：1μL.
Column flow：1.5mL/min.
Make-up gas flow 4mL/min.
Temperature is set：Split ratio is 20: 1, and the bypass flow is 30mL/min；The column flow is 1.5mL/min, institute
It is 5mL/min to state make-up gas flow, and the sample size is 1.0 μ L；The injector temperature is 230 DEG C, the detector temperature
For 250 DEG C；Column temperature is heated up using three ranks, and 1) 40 DEG C of initial temperature, keep 2min；2) 60 DEG C are risen to 5 DEG C/min heating rate, protected
Hold 0min；3) 90 DEG C are risen to 15 DEG C/min heating rate, keeps 0min；4) 140 are risen to 25 DEG C/min heating rate
DEG C, keep 0min.
2nd, standard liquid is prepared
5ml stripping liquids are added in 10ml parsing bottles, weigh about 10mg styrene chromatographically pure and about 2mg acrylonitrile respectively
Chromatographically pure is added in the parsing bottle, is added stripping liquid and is diluted to scale, the polystyrene standards that preparation obtains 1000 μ g/mL are molten
Liquid and 200 μ g/mL acrylonitrile standard liquids.Solution concentration is calculated by constituent mass and stripping liquid stereometer, this solution is store for standard
Standby liquid.Or prepared with the standard liquid of authoritative institution's assignment.Wherein, standard working solution is diluted by standard liquid and is made.
3rd, sample collection
Spot sampling performs according to GBZ 159-2004, GBZ/T 160.68-2007 and GBZ/T 160.42-2007.
1) short time samples：Activated carbon tube both ends are opened in sampled point, the activated carbon tube is connected with the air sampler,
With 100ml/min flow collection 15min air samples.
2) sample for a long time：Activated carbon tube both ends are opened in sampled point, the activated carbon tube is connected with the air sampler,
With 50ml/min flow collection 2h-8h air samples.
3) personal sampling：Activated carbon tube both ends are opened in sampled point, the activated carbon tube is connected with the air sampler, are worn
The shirtfront top of sample objects is worn over, as far as possible close to breathing zone, with 50ml/min flow collection 2h-8h air samples.
4) sample blank：The activated carbon tube is not connected to the air sampler, and activated carbon tube is brought to sampled point, remaining operation
Step is the same as 1), 2) or 3).
After the completion of sampling, closing activity charcoal pipe both ends, put transport in cleaning container and preserve, sample at room temperature may be used immediately
Preserve 5d.
4th, determine the standard liquid and draw standard curve
Standard working solution, minimum 5 concentration of standard working solution are diluted to standard liquid.It will be marked with micro syringe
In quasi- working solution injecting chromatograph, parallel determination number is 3 times, you can corresponding peak height value or peak area value is obtained, to survey
The peak area average obtained draws standard working curve, the phase relation of regression equation to corresponding styrene or the fine concentration of propylene respectively
Number should be greater than 0.99.Standard curve regression equation is as follows：
Y=ax+b
In formula：X is standard liquid concentration, g/L；
Y is that each standard liquid concentration corresponds to peak area, pA*min；
A is standard curve regression equation slope；
B is standard curve regression equation intercept.
5th, sample solution is prepared
The sample solution includes air sample solution and sample blank solution.The Activated charcoal tube of air sample will be gathered
Both ends are poured into parsing bottle respectively, are added stripping liquid, closing shaking, are produced sample solution.The activity of sample blank will be gathered
The both ends of carbon pipe are poured into parsing bottle respectively, are added stripping liquid, closing shaking, are produced sample blank solution.
6th, determination sample
Using with determine the standard liquid identical condition determination, respectively by the air sample solution and the sample blank it is molten
Liquid is injected into the capillary chromatography and is measured, and respectively obtains the peak height value or peak area value and sample sky of the air sample
White peak height value or peak area value.The peak height value or peak area value of the air sample are subtracted to the peak height value or peak of the sample blank
Area value, styrene in air or the fine content of propylene are obtained by standard curve.Sample concentration is calculated as follows formula calculating.
In formula：X be stripping liquid in each component concentration, μ g/mL；
Y is component peak area to be measured, pA*min；
A is standard curve regression equation slope；
B is standard curve regression equation intercept.
, can direct-reading sample size if the automatically derived sample concentration of software.
7th, the amendment of result
1) when workplace air sample sampling volume in sampled point temperature less than 5 DEG C and higher than 35 DEG C, atmospheric pressure
During less than 98.8KPa and higher than 103.4KPa, sampling volume should be converted into standard sample volume as the following formula.
In formula：Vo is standard sample volume, L；
V is sampling volume (sampling flow is multiplied by the sampling time), L；
T is the temperature of sampled point, DEG C；
P be sampled point atmospheric pressure, kPa.
2) benzene in air ethene or the fine concentration of propylene is calculated as follows.
In formula：C1, c2 are to measure concentration of component (subtracting sample blank), g/ml in front and rear section adsorbent stripping liquid；
C be sample in concentration of component, mg/m3；
V0For standard sample volume, L；
V be stripping liquid volume, ml；
D is desorption efficiency, is calculated by every batch of adsorption tube practical measurement result.
3) the time weight mean exposure concentration of styrene and acrylonitrile presses GBZ159-2004 rule in workplace air
Devise a stratagem is calculated.
Effete test embodiment
It is measured using the method 1 of styrene and acrylonitrile content in translocation workplace air in embodiment 1.
1st, the drafting of standard curve
It is serial into standard working solutions more than 5 concentration units with stripping liquid working solution.Using the institute of embodiment 1
The chromatographic condition shown, capillary chromatography is adjusted to optimum determining state, sample introduction 1ml, difference metric works solution system
Row, each concentration replication 3 times.Standard curve is drawn to concentration with the peak height value or peak area average that measure.Styrene mark
Directrix curve regression equation is：Y=51.1224x-0.0180, r=0.9999；Acrylonitrile standard curve regression equation is：Y=
40.7507x+0.0610 r=0.9999.
2nd, the confirmation of detection limit
Detection limit is under certain confidence level, and assay method can measure the least concentration or amount of test substance, this experiment
Using standard deviation method, confidence level 99%, a certain amount of test substance is added, and dosage is more than detection limit, again less than 10 times
Detection limit.Carry out the measure of 10 parallel samples, in this method the detection of styrene be limited to 0.535g/L；Acrylonitrile in this method
Detection be limited to 0.269g/L.To sample the calculating of 6L air samples, styrene concentration limit is 0.09g/m3；Acrylonitrile is most
Low concentrations are 0.05g/m3。
3rd, measurement range
The standard curve range of styrene is 0 μ g/mL-1082.9 μ g/mL in this method, be can be identified as with reference to limit is quoted
2.14 μ g/mL-1082.9 μ g/mL, the standard curve range of acrylonitrile is 0 μ g/mL-207.38 μ g/mL, can be true with reference to limit is quoted
It is set to 1.08 μ g/mL-207.38 μ g/mL.The r=0.9999 of standard curve within this range.
4th, it is repeated
In linear scope, the sample of high, medium and low various concentrations is measured using this method, wherein, styrene
Concentration is respectively 1000 μ g/mL, 500 μ g/mL and 50 μ g/mL, acrylonitrile concentration be respectively 200 μ g/mL, 100 μ g/mL and
25 μ g/mL, as a result show that the relative standard deviation of styrene exists in 0.51%-1.33%, the relative standard deviation of acrylonitrile
0.21%-1.92%, it disclosure satisfy that GBZ/T210.4-2008 requirement.
5th, Intermediate precision
This method includes sample treatment and measure overall process.High, medium and low 3 in the range of selection standard curve determination
Concentration, 6 replications were carried out in -5 days 3 days, calculate its relative standard deviation.Experiment finds that the RSD of styrene measure exists
0.63%-2.49%, the RSD of acrylonitrile measure disclosure satisfy that GBZ/T 210.4-2008 requirement in 2.05%-4.08%.
6th, the degree of accuracy
With the standard liquid of national assignment, being diluted to the blind samples of high, medium and low various concentrations certainly, (concentration of styrene is about
1000,500,50 μ g/mL, acrylonitrile concentration are about 200,100,25 μ g/mL) sample introduction measure.Styrene determines in this method
Average recovery of standard addition be 97.66%-99.77%, and the average recovery of standard addition of acrylonitrile measure is 96.09%- in this method
97.74%, it disclosure satisfy that GBZ/T 210.4-2008 requirement.
7th, the experiment of sample stability
This method uses the standard liquid from dilution, is added in activated carbon tube, the amount of added determinand is in assay method
In measurement range.Closed placement at room temperature, respectively on the day of, the 3rd day, the 5th day, the 7th day, the 9th day, the 11st day, the 13rd day,
Respectively determine 6 samples within 15th day.The number of days of rate of descent≤10% is stabilization time.The acrylonitrile sample that this method finds to adopt back exists
It can preserve at room temperature more than 7 days, and the styrene sample adopted back can preserve more than 15 days at room temperature.
8th, conclusion
The detection of 8.1 styrene
The detection of this method is limited to 0.535 μ g/mL, and in terms of gathering 6L air samples, then concentration limit is 0.09mg/
m3.Precision is 0.51~1.33%, and the range of linearity is 2.14 μ g/mL-1082.9 μ g/mL, and the sample adopted back is steady at normal temperatures
It is qualitative to be more than 15 days.
The detection of 8.2 acrylonitrile
The detection of this method is limited to 0.27 μ g/mL, and in terms of gathering 6L air samples, then concentration limit is 0.04mg/
m3.Precision is 2.05%~4.08%, and the range of linearity is 1.08 μ g/mL-207.38 μ g/mL, and the sample adopted back is at normal temperatures
Stability is more than 5 days.
The translocation of 8.3 benzene homologues
As shown in figure 1, this method there are about 6min from acetone appearance time to styrene appearance time, as contained it in air
His benzene homologues can appearance in this time difference, so as to not Interference Detection.Therefore this method can be applied to benzene homologues and propylene
The translocation of nitrile.
The method of styrene and acrylonitrile content from the translocation workplace air of the above results showed that present invention
Every the result meet standard requirement, meet GBZ/T210.4-2008《Occupational health standard formulation guide》Middle regulation
Requirement.
And relative to the method in traditional GBZ/T160.42-2007 and GBZ/T160.68-2007 to styrene and third
Alkene nitrile is sampled and determined, it is necessary to sampled respectively, and is individually detected, can not realize in workplace air styrene and
The translocation of acrylonitrile content.The detection efficiency of conventional method is relatively low, and operation is more complicated.
Therefore, the method for styrene and acrylonitrile content is simple and convenient in translocation workplace air of the invention, detection
Efficiency high, and comply with the national standard requirements.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of method of styrene and acrylonitrile content in translocation workplace air, it is characterised in that using capillary color
Spectrometer determines, and comprises the following steps：Standard liquid is prepared, sample is gathered, prepares sample solution, determine the standard liquid and paint
Standard curve processed and the measure sample solution；
Wherein, the chromatographic condition of the capillary chromatography measure is：Capillary chromatographic column is polarity capillary column；Detector is
Hydrogen flame ionization detector；Using split sampling mode, split ratio 20: 1, the bypass flow is 30mL/min；The post
Flow is 1.5mL/min, and the make-up gas flow is 5mL/min, and the sample size is 1.0 μ L；The injector temperature is 230
DEG C, the detector temperature is 250 DEG C；The initial column temperature is 40 DEG C, keeps 2min, column temperature is with 5 DEG C/min heating rate
60 DEG C are warming up to, then 90 DEG C are warming up to 15 DEG C/min heating rate, is finally warming up to 140 with 25 DEG C/min heating rate
℃。
2. the method for styrene and acrylonitrile content in translocation workplace air according to claim 1, its feature exists
In the carrier gas of the capillary chromatography is high pure nitrogen.
3. the method for styrene and acrylonitrile content in translocation workplace air according to claim 1, its feature exists
In the polarity capillary column is FFAP polarity capillary columns.
4. the method for styrene and acrylonitrile content in translocation workplace air according to claim 4, its feature exists
In model 30m × 0.32mm × 1.0 μm of the FFAP polarity capillary column.
5. the method for styrene and acrylonitrile content in the translocation workplace air according to claim any one of 1-4,
Characterized in that, described the step of preparing standard liquid, includes：5ml stripping liquids are added in 10ml parsing bottles, weighed respectively
10mg styrene chromatographically pure and 2mg acrylonitrile chromatographically pures are added in the parsing bottle, are added stripping liquid and are diluted to scale, respectively
Preparation obtains the standard liquid and 200 μ g/mL acrylonitrile standard liquids of 1000 μ g/mL styrene.
6. the method for styrene and acrylonitrile content in the translocation workplace air according to claim any one of 1-4,
Characterized in that, the step of collection sample, includes：Activated carbon tube is connected with air sampler, and opens and lives in sampled point
Property charcoal pipe both ends, sampled by the short time, for a long time sampling or personal sampling collection air sample；Again by the activated carbon tube with
The air sampler separation, to gather sample blank；The complete closing activated carbon tube both ends, are placed in cleaning and hold after the completion of sampling
Transport and preservation in device；Wherein, the step of short time sampling includes：The both ends of the activated carbon tube are opened in sampled point,
The activated carbon tube is connected with the air sampler, with 100ml/min flow collection 15min air samples；When described long
Between sample the step of include：The both ends of the activated carbon tube are opened in sampled point, by the activated carbon tube and the air sampling
Device is connected, with 50ml/min flow collection 2h-8h air samples；The step of personal sampling, includes：Institute is opened in sampled point
The both ends of activated carbon tube are stated, the activated carbon tube is connected with the air sampler, is worn on the shirtfront top of sample objects,
Close to breathing zone, with 50ml/min flow collection 2h-8h air samples；The step of collection sample blank, includes：Sampling
Point opens the both ends of the activated carbon tube, and Activated charcoal tube is not connected to the air sampler, and remaining step is adopted with the short time
The step of sample, long-time sampling or personal sampling, is identical.
7. the method for styrene and acrylonitrile content in the translocation workplace air according to claim any one of 1-4,
Characterized in that, the sample solution includes air sample solution and sample blank solution；Prepare the air sample solution
Step includes：The both ends for the Activated charcoal tube for gathering air sample are poured into parsing bottle respectively, add stripping liquid, closing is shaken
Shake, produce air sample solution；The both ends for the Activated charcoal tube for gathering sample blank are poured into parsing bottle respectively, add solution
Imbibition, closing shaking, produces sample blank solution.
8. the method for styrene and acrylonitrile content in the translocation workplace air according to claim any one of 1-4,
Characterized in that, described determine the standard liquid and include the step of drawing standard curve：The standard liquid is injected into
The capillary chromatography is measured, and is repeated three times, and corresponding peak height value or peak area value is respectively obtained, with described
Peak height value or the average of peak area value draw standard curve to corresponding styrene-content or the fine content of propylene respectively.
9. the method for styrene and acrylonitrile content in the translocation workplace air according to claim any one of 1-4,
Characterized in that, determining the sample solution includes measure air sample solution and determination sample blank solution, specific steps bag
Include：Using with determining the standard liquid identical condition determination, respectively by the air sample solution and the sample blank
Solution is injected into the capillary chromatography and is measured, and respectively obtains the peak height value or peak area value and sample of air sample
The peak height value or peak area value of blank, the peak height value of the air sample are subtracted the peak height value of the sample blank, or by institute
The peak area value for stating air sample subtracts the peak area value of the sample blank, by the standard curve obtain in air styrene or
The fine content of propylene.
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